HRID2368778

反应详情

EQUATION

反应方程式

HRID 2368778 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Stannous chloride dihydrate (3.6 g, 16 mmol) was dissolved in 10 mL of concentrated hydrochloric acid. The solution was added to N-(2-methyl-5-nitrophenyl)-4,5′-bipyrimidin-2-amine with violent stirring. The mixture was poured into ice-cold water after being stirred for 2 hours. It was then neutralized to pH>8 with sodium carbonate and extracted with ethyl acetate for 4 times. The pooled extracts were washed with brine, dried over magnesium sulfate and finally concentrated under reduced pressure to obtain 0.7 g of the title compound. MS (M+1)=279.13.

WORKUP

后处理

  1. additionThe mixture was poured into ice-cold water
  2. extractionextracted with ethyl acetate for 4 times
  3. washThe pooled extracts were washed with brine
  4. dry with materialdried over magnesium sulfate
  5. concentrationfinally concentrated under reduced pressure